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Critical Reviews in Food Science and Nutrition

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A review of encapsulation of carotenoids usingspray drying and freeze drying

Jong-Bang Eun, Ahmed Maruf, Protiva Rani Das & Seung-Hee Nam

To cite this article: Jong-Bang Eun, Ahmed Maruf, Protiva Rani Das & Seung-Hee Nam (2019):A review of encapsulation of carotenoids using spray drying and freeze drying, Critical Reviews inFood Science and Nutrition, DOI: 10.1080/10408398.2019.1698511

To link to this article: https://doi.org/10.1080/10408398.2019.1698511

Published online: 26 Dec 2019.

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REVIEW

A review of encapsulation of carotenoids using spray drying and freeze drying

Jong-Bang Eun, Ahmed Maruf�, Protiva Rani Das�, and Seung-Hee Nam

Department of Food Science and Technology and BK 21 Plus Program, Graduate School of Chonnam National University, Gwanju,South Korea

ABSTRACTCarotenoids are potent antioxidants, but they are highly unstable and susceptible during process-ing and storage. Encapsulation technologies protect against degradation and are capable ofreleasing individual or combination of bioactive substances during processing as well as develop-ment of various functional food products. Moreover, encapsulating agents can be used to increasethe stability of carotenoids and form a barrier between the core and wall materials. Suitableencapsulating agents, temperature, and drying methods are the most important factors for theencapsulation process. In this report, we reviewed the current status of encapsulation of carote-noids from different fruits, vegetables, spices, seaweeds, microorganisms, and synthetic sourcesusing various types of encapsulating agents through spray drying and freeze drying. We alsofocused on the degradation kinetics and various factors that affect the stability and bioavailabilityof encapsulated carotenoids during their processing and storage.

KEYWORDSCarotenoids; encapsulation;spray drying; freeze drying;fruits; vegetables

Introduction

Carotenoids, the main sources of vitamin A, are useful inpreventing degenerative human diseases because of theirantioxidative and free radical scavenging properties (Kimet al. 2006; Krishnaiah, Sarbatly, and Nithyanandam 2011).b-carotene, a-carotene, and b-cryptoxanthin lycopene,lutein, and its isomer zeaxanthin are known as carotenoids(McGuire and Beerman 2007). The human body is not cap-able of synthesizing carotenoids; therefore, carotenoids mustbe supplied through the diet. Natural antioxidants haveattracted considerable attention because of their safety incomparison with artificial antioxidants. Natural antioxidantscan be added to different food products in different ways.They can be used to increase stability by preventing lipidperoxidation, thereby increasing the shelf life of food prod-ucts. Recently, there has been a global trend of using phyto-chemicals from natural sources, such as vegetables, fruits,oilseeds, and herbs, as antioxidants and functional ingre-dients (Elliott 1999; Kaur and Kapoor 2001). However, it isvery difficult to store fruits and vegetables for a long timebecause of their perishable nature, even at low temperatures.Elevated temperature, light, oxygen, and pH are parametersthat affect the degradation of phytochemicals (Xianquanet al. 2005). Therefore, processing is necessary to prolongthe shelf life. Drying is one of the oldest food preservationtechniques, and among all drying methods, spray drying,and freeze drying are two of the best methods for preservingbioactive compounds. Spray dryers and freeze dryers arewidely used to produce dried fruits and vegetables, and they

can preserve heat-sensitive bioactive components, such asphenolic compounds, carotenoids, and anthocyanins, moreeffectively than other drying methods.

Encapsulation technology is used in the food industry todevelop liquid and solid ingredients as effective barriers againstenvironmental parameters, such as oxygen, light, and free radi-cals (Desai and Park 2005). Bioactive compounds can beimproved by using encapsulation techniques, which entrap sen-sitive ingredients inside a coating material (Saenz et al. 2009).Moreover, encapsulating agents can be used to increase the sta-bility of bioactive compounds. Researchers (Saenz et al. 2009;Ahmed et al. 2010a; Ahmed et al. 2010b; Kha, Nguyen, andRoach 2010) have used various encapsulation materials, such asstarch, maltodextrin, corn sirup, inulin, and Arabic gum toimprove bioactive compounds during spray drying. Somereviews on encapsulation techniques, such as microencapsula-tion of oils (Bakry et al. 2016) and microencapsulation of vita-min A (Goncalves, Estevinho, and Rocha 2016), exist.However, these reviews lack information regarding the selectionof encapsulating materials and modeling for encapsulation ofcarotenoids. Therefore, the objective of this review is to illus-trate the impact of encapsulating agents on carotenoids fromdifferent sources, as well as the degradation kinetics duringprocessing and storage using spray dryers and freeze dryers.

General characteristics of carotenoids

Carotenoids are isoprenoid compounds. More than 600 dif-ferent fat-soluble carotenes have been isolated from plants

CONTACT Jong-Bang Eun jbeun@jnu.ac.kr Department of Food Science and Technology and BK 21 Plus Program, Graduate School of Chonnam NationalUniversity, Gwanju South Korea.Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/bfsn.�Both authors are equally contributed.� 2019 Taylor & Francis Group, LLC

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITIONhttps://doi.org/10.1080/10408398.2019.1698511

(Gul et al. 2016). The chemosynthesis of carotenoidsinvolves tail-to-tail linkage of two C20 geranyl-geranyldiphosphate molecules, resulting in a progenitor C40 carbonskeleton from which all individual variations are derived(Figure 1) (Dutta, Raychaudhuri, and Chakarborty 2005).b-carotene, lutein, zeaxanthin, neoxanthin, vioxanthin, andchlorophylls are the most commonly found carotenoids inplants (Gul et al. 2016; Lakshminarayana et al. 2005).b-carotene (chemical formula, C40H56; molecular weight,536.88 g/mol) is widely distributed in plant based foods andmicroorganisms (Khachik, Beecher, and Smith 1995).Generally, all transb-carotenes are dominant precursors ofvitamin A (Krinsky and Johnson 2005). The physicochemi-cal features including color, chemical reactivity, molecularshape, light absorbing intensity, and antioxidant propertiesof carotenoids depend on the length of the polyene chain(Figure 2) (Britton 1995; Dutta, Raychaudhuri, andChakarborty 2005). Carotenoids are classified into two cate-gories: (i) alpha-, beta-, gamma-carotene and alpha-, beta-cryptoxanthin, which can be metabolized by humans intoretinol, and (ii) lutein, zeaxanthin, lycopene, which are unre-lated to any vitamin A activity in humans (Bohn 2008).

A number of factors are responsible for the degradation ofcarotenoids. On exposure to heat, light, and oxygen duringprocessing and storage, trans-b-carotene immediately under-goes thermal and chemical oxidation, isomerization, and pho-tosensitization (Figure 3) (Dutta, Raychaudhuri, andChakarborty 2005; Gul et al. 2016). The instability of carote-noids is caused by their structural polyene chain. The oxidationprocess of carotenoids involves epoxidation, forming apocaro-tenoids (Marty and Berset 1988), and low molecular weightcompounds responsible for the off-flavor in food (Falconeret al. 1964). During digestion, carotenoids also degrade in vari-ous ways in the human body (Figure 4). Therefore, retentionof carotenoids is a major issue during their processing andstorage. Microencapsulation techniques could enhance the

retention of carotenoids during processing and storage andprotect against degradation from light, heat, and temperature.

General aspects of microencapsulation

The encapsulation technique is widely used in several fields,particularly in the food industry (Higuera-Ciapara et al.2004; Shen and Tang 2012). The process involves coating orentrapping solid, liquid, or gas particles into thin films usingvarious food-grade encapsulating agents (Gharsallaoui et al.2007; Goncalves, Estevinho, and Rocha 2016). During encap-sulation, the core materials are surrounded by a wall, whichacts as a physical barrier to protect them from external fac-tors. The coating material, encapsulating agents, carrier,shell, capsule, membrane, packaging material, or the externalphase, are known as wall materials. Core materials are alsocalled core actives, fills payloads, or the internal phase. Theparticles obtained are called microcapsules. Most micro-capsules are small spheres with diameters ranging betweenmicrometers and millimeters. The sizes and shapes of themicroparticles depend on the materials and methods used toprepare them (Gharsallaoui et al. 2007). Some microcapsulesmay have multiple microencapsulating agents that form dif-ferent walls with different chemical and physical properties(Botelho et al. 2007). The morphology of microcapsulesdepends mainly on the core materials and depositionprocess of the shell. Various microcapsules are shown inFigure 5. The main purposes of the encapsulation processin the food industry are given below:

i. Reducing the transfer rate of the core materials to thesurrounding materials.

ii. Protecting the core materials from undesirableenvironmental conditions.

iii. Preventing incompatibility and reactivity ofthe compounds.

iv. Modifying the physical characteristics of the originalmaterials for easy handling.

v. Masking undesirable taste or unwanted aroma of thecore materials.

vi. Diluting the core materials to decrease quantity of thecompound when desirable.

vii. Controlling the release of core materials.viii. Providing better storage conditions by preventing

degradative reactions like dehydration and oxidation.

Common microencapsulating agents

Encapsulation efficiency and microcapsule stabilitydepend on the encapsulating agent or wall material.

Figure 1. Structure of b-carotene.

Figure 2. Physical and chemical properties of carotenoids.

2 J.-B. EUN ET AL.

Therefore, selecting appropriate encapsulating agentsis necessary to maintain the desirable encapsulationefficiency, microparticle stability, and the requiredcharacteristics of the final product (Goncalves, Estevinho,and Rocha 2016). The wall material can be selected from

a wide variety of natural and synthetic polymers.Different types of encapsulating agents are used as wallmaterials during spray and freeze drying. In this review,we focus on encapsulating agents that are commonly usedduring spray drying and freeze drying.

Figure 3. Diametric presentation of carotenoids degradation.

Figure 4. Degradation way of lycopene in human body (adapted from Bohn 2008).

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 3

Maltodextrins

Maltodextrins are polysaccharides and water-soluble materi-als, available as white powders. Maltodextrins are usuallyclassified by their dextrose equivalent value (DE) (Desobry,Netto, and Labuza 1999). Maltodextrins with DE values of 4,10, 15, 20, 25, 30, and 42 are available in the market.Maltodextrins are commonly used as encapsulating agentsfor freeze drying, and are also often used in various sugar-rich foods such as blackcurrant, raspberry, and apricot juiceduring spray drying. Addition of maltodextrins during thedrying process increases the glass transition temperature andreduces stickiness of the product (Quek, Chok, andSwedlund 2007). Maltodextrins help in retaining certainproduct properties, such as nutrient content, color, and fla-vor during drying (Rodriguez-Hernandez et al. 2005).

Starch

Starch is soluble in water and can be separated into its com-ponent fractions, amylose and amylopectin, by heating. Dueto its qualities, such as abundant availability, low cost, andemulsifying properties during drying starch has been widelyused as a wall material. Starch has also been used toenhance storage stability of flavors (Partanen et al. 2002).Different types of starches are used as encapsulating agentsduring drying: modified tapioca starch, native tapioca starch,and waxy maize starch. However, some studies (Bayram,Bayram, and Tekin 2005; Gharsallaoui et al. 2007) havereported that starch is not a suitable encapsulation agentduring spray drying because it caramelizes, attaches to thespray-dryer wall, and clogs the nozzle due to its heteroge-neous form during drying.

Gum Arabic

Gum Arabic, also known as acacia gum, is composed of pol-ysaccharides and glycoproteins. It is often used as an effect-ive encapsulating agent because of its protective colloidfunctionality (Krishnan, Bhosale, and Singhal 2005). Duringspray drying, gum Arabic is used as an encapsulating agent

to obtain good emulsifying capacity and low viscosity in anaqueous solution. Gum Arabic is 3 to 4 times more stablethan maltodextrin in bixin encapsulation (Barbosa,Borsarelli, and Mercadante 2005). However, it not as effect-ive as other wall materials, such as citral, linalool, b-myr-cene, limonene, and b-pinene (Bertolini, Siani, andGrosso 2001).

Chitosan

Chitosan is a linear polysaccharide, which is soluble inacidic aqueous media. The application of chitosan as a coat-ing material is increasing because of its biocompatibility,low toxicity, and biodegradability (Grenha et al. 2007).Chitosan alone, rather than a combination of chitosan andmaltodextrin, is unable to provide a stable emulsion for fishoil-encapsulated powders after freeze drying (Klaypradit andHuang 2008).

Inulin

Inulin is a polysaccharide that is produced by many types ofplants, such as chicory (Cichorium intybus) root, dahlia(Dahlia pinnata Cav.), and Jerusalem artichoke (Helianthustuberosus). Inulin is an excellent potential encapsulatingagent because of its low cost and nutritive properties(Stevens, Meriggi, and Booten 2001). Gandomi et al. (2016)demonstrated that chitosan-coated alginate beads increasedbacterial survival in stored apple juices. A mixture of inulinand whey protein isolate was a suitable carrier for the spraydrying of rosemary essential oil (Fernandes et al. 2014).

Proteins

Different types of proteins, such as soy protein, whey pro-tein, and gelatin, are used in the food industry as carrieragents. Among them, soy protein is one of the most popularplant protein sources because it is abundant and inexpen-sive. During spray drying, proteins are used as encapsulatingmaterials because they protect against oxidation (Bylaiteet al. 2001) and have high-binding properties (Landy,Druaux, and Voilley 1995). Pea protein could be used as agood carrier agent for the microencapsulation of ascorbicacid (Pierucci et al. 2006). Vega et al. (2005) showed thatsodium caseinate showed better encapsulation propertiesthan micellar casein.

Ascorbic acid

Ascorbic acid, known as vitamin C, is a white or light-yel-low powder. Many researchers have used ascorbic acid as aprotective agent during spray drying (Ahmed et al. 2010a;Desai and Park 2005). Ascorbic acid has the ability toreduce hygroscopicity and dusting, and it provides a highdegree of flowability without clumping during the encapsu-lation process (Shahidi and Han 1993).

Figure 5. Different types of microcapsules: (i) simple microcapsule, (ii) matrix(microsphere), (iii) irregular microcapsule, (iv) multicore microcapsule, (v) multi-wall microcapsule, and (vi) assembly of a microcapsule (adapted from Bakryet al. 2016).

4 J.-B. EUN ET AL.

Other encapsulation agents

The above-mentioned wall materials have been widely usedduring drying. However, some researchers have also useddifferent wall materials, such as carrageenan, silicon dioxide,sodium caseinate, soy lecithin, and sodium alginate.

Encapsulation techniques

Numerous techniques are used for the encapsulation processin the food industry. Encapsulation techniques can be classi-fied as follows (Munin and Edwards-L�evy 2011): Physicalmethods: spray drying, fluid bed coating, extrusion-sphero-nization, centrifugal extrusion, pan coating, drum drying,freeze drying, and processes using supercritical fluids.

Physicochemical methods: spray cooling, hot meltcoating, ionic gelation, solvent evaporation extraction, andsimple or complex coacervation.

Chemical methods: interfacial polycondensation, in situpolymerization, interfacial polymerization, and interfacialcross-linking.

Spray drying is the simplest and oldest used commercialmethod for encapsulation (Shahidi and Han 1993). Freezedrying could also be used to obtain bioactive compoundsduring encapsulation. Therefore, in this review, we focuson the encapsulation of carotenoids from fruits, vegetables,spices, seaweed microorganisms, and synthetic sources usingspray and freeze drying.

Spray drying technology

Spray drying has been widely used in the food industry forcommercial production of dried fruits and vegetables. Spraydrying is highly appropriate for heat-sensitive food ingre-dients. Various stages are involved in the encapsulation pro-cess using spray drying (Figure 6). The encapsulationefficiency depends on a number of factors, such as the feedflow rate, air inlet/outlet temperature, feed temperature, and

wall materials (Bakry et al. 2016). The working principles ofspray drying are as follows: first, mixtures are fed throughpipes and atomized by a nozzle. Then, water is removedfrom the solution using hot air, and dried powderis obtained at the bottom of the dryer (Bakry et al. 2016).The advantages of spray drying include good reconstitu-tional characteristics, low water activity, and suitability fortransport and storage. However, scarcity of good wall mate-rials, as well as agglomeration properties of the microcapsulepowder, are the limitations of spray drying during theencapsulation process. Carotenoid stability in foods suchas carrot, sweet potato, tomato, and melon using differentwall materials has been examined during spray drying(Kha, Nguyen, and Roach 2010).

Freeze drying technology

Freeze drying is also called lyophilization, and the process isshown in Figure 7. Sublimation is the main principle of thefreeze-drying process. During sublimation, water is directlyconverted to vapor without passing through the liquid statein vacuum (Bakry et al. 2016). Freeze drying has alreadybeen successfully used for encapsulation to maintain nutri-tional factors and facilitate drying. Velasco, Dobarganes, andM�arquez-Ruiz (2003) revealed that encapsulated freeze-driedsamples were more resistant to oxidation and protectedfrom heat-sensitive core materials. However, long processingtimes, high energy, and high production cost are the maindrawbacks of freeze drying (Bakry et al. 2016).

Effects of encapsulation agents applied for differentcarotenoids

Impact of various encapsulating agents on differentcarotenoids through spray and freeze drying are shownin Tables 1–3.

Encapsulation of carotenoids using maltodextrins andpolysaccharides

Table 1 shows the encapsulation of carotenoids usingmaltodrstring and polysaccharides. Kha, Nguyen, and Roach(2010) and Angkananon and Anantawa (2015) observed thatlower concentration of maltrodextrin (10%) retained higher

Figure 6. Schematic representation of the microencapsulation process by spraydrying (adapted from Bakry et al. 2016).

Figure 7. Schematic diagram of a freeze dryer (adapted from Bakry et al. 2016).

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 5

amount of total carotenoid content in gac fruit powderthan those of higher concentration of maltrodextrin (30%).Pequi was encapsulated with maltodextrin (15% to 30%) bySantana et al. (2016), who reported that a maltodextrinconcentration of 18% retained the maximum amount oftotal carotenoids during spray drying. The results showedthat higher concentrations of maltodextrin hindered theformation of emulsion, possibly reducing the protectiveeffect of carotenoids. Shishir et al. (2016) prepared guavapowder using 10% and 20% maltodextrin and found thatthe lycopene content increased with increasing maltodextrinconcentrations. Grabowski, Truong, and Daubert (2008)produced flour from yellow-fleshed sweet potatoes by usingmaltodextrin and spray drying. They revealed that b-caro-tene contents of maltodextrin-treated powder and untreated

powder were significantly different, and that isomerizationand loss of b-carotene were also higher in the maltodextrin-treated powder than in the control. Wagner and Warthesen(1995) also used 4, 15, 25, and 36.5 DE maltodextrinto produce spray-dried carrot powder. They concludedthat 36.5 DE maltodextrin showed maximum retention ofa-carotene and b-carotene, and could, thus, possible providebest protection from oxidation. Carrot juice preparedwith maltodextrin had a 70–220 times higher shelf-life thancarrot juice produced without maltodextrin (Wagner andWarthesen 1995). The authors hypothesized that the carrieragents might prevent oxidation. Quek, Chok, and Swedlund(2007) also found maltodextrin treated water melon powderhad more lycopene and b-carotene contents than rawwatermelon juice. Hojjati et al. (2011) revealed that

Table 1. Encapsulation of carotenoids using maltodextrins and others polysaccharides.

Sources of carotenoids Drying conditions Carrier agents Compounds References

Gac fruit (Momordicacochinchinensis)

Inlet temperature: 120 �C, 140 �C,160 �C, 180 �C, 200 �C

Outlet temperature: 83 �C, 94 �C,103 �C, 112 �C, 125 �C

Air flow rate: 56 ± 2 m3/hCompressor air pressure: 0.06MPa

gaugeFeed rate was constant:12–14mL/min

12 DE maltodextrin (10%,20%, and 30% w/v)

Total carotenoid content Kha, Nguyen, and Roach(2010)

Gac fruit (Momordicacochinchinensis

Spreng)

Inlet temperature: 120 �C, 150 �C,170 �C

Outlet temperature: 66 �C, 74 �C,88 �C

100% aspirator, 30–40% pump and30–40 Q-flow

Maltodextrin (10%, 20%, and30% w/v)

b-carotene and lycopene Angkananon and Anantawa(2015)

Pequi (Caryocarbrasiliense Camb.)

Inlet temperature: 140 to 200 �COutlet temperature: 99 to140 �C

Air flow rate: 0.6 m3/hFeed flow rate: 0.2 kg/h

10 DE maltodextrin (15%,18%, 22.5%, 27%, and30% w/v))

Total carotenoids Santana et al. (2016)

Pink guava (Psidium guajava) Inlet temperature: 150 �C, 160 �C,170 �C

Outlet temperature: 90 ± 2 �CAir flow rate: 47 ± 2 m3/hFeed flow rate: 350 to 500mL/hPressure: 2.1 ± 1 bar

10 DE maltodextrin (10% and20% w/v))

Lycopene Shishir et al. (2016)

Sweet potatoes(Ipomoea batatas)

Inlet temperature: 190 �COutlet temperature: 100 �CFeed temperature: 60 �C

11 DE maltodextrin (10 g/100 g of puree)

b-carotene and all transforms and cis formsof b-carotene

Grabowski, Truong, andDaubert (2008)

Carrot (Daucus carota L.) Inlet temperature: 200 ± 5 �COutlet temperature: 100 ± 5 �C

4, 15, 25, and 36.5 DEmaltodextrin

b-carotene and a-carotene Wagner and Warthesen (1995)

Watermelon (Citrullus lanatus) Inlet temperature: 145 �C, 155 �C,165 �C

175 �C, Aspirator rate: 60%Flow rate: 600 L/h, Pressure: 4.5 barFeed temperature: 20 �C

Maltodextrin (3 and 5% w/v) b-carotene and Lycopene Quek, Chok, and Swedlund(2007)

Dietzia natronolimnaea HS-1 Inlet temperature: 170 ± 2 �COutlet temperature: 90 ± 2 �CAir pressure: 0.5MPaFeed flow rate: 300mL/min

10% (w/v) soluble soybeanpolysaccharide suspensionin distilled water at 0.25,0.50,

0.75, and 1.00 ratios.

Canthaxanthin Hojjati et al. (2011)

Trans-b-carotene Freeze drying 6 DE starch, 12 DE starch andnative starch

b-carotene Spada et al. (2012)

Pequi (Caryocarbrasiliense Camb.)

Inlet temperature: 140 to 200 �COutlet temperature: 82 to 115 �CAir flow rate: 0.6 m3/hFeed flow rate: 0.2 kg/h

Modified starch (15%, 18%,22.5%, 27%, and 30% w/v)

Total carotenoids Santana et al. (2014)

Black pepper (Piper nigrum) Inlet temperature: 178 �COutlet temperature: 110 �CFeed flow rate: 300mL/min

40 g gum Arabic andcommercialmodified starch

Oleoresin Shaikh, Bhosale, and Singhal(2006)

Trans-b-carotene Freeze drying Almond gum and gum Arabic b-carotene Mahfoudhi and Hamdi (2015)Tomato (Lycopersicon

esculentum Mill.)Freeze drying 1:1 and 1:4 (w/w) of

lycopene and b cyclodextrinLycopene Nunes and Mercadante (2007)

6 J.-B. EUN ET AL.

oxidation of canthaxanthin was lower in the microcapsulesthan that in the non encapsulated control. Trans-b-carotenewas prepared with native starch, 6 DE starch, and 12 DEstarch by freeze drying (Spada et al. 2012). The resultsshowed that hydrolyzed starch could retain b-carotene betterthan native starch, due to variation in sizes of particles.Spada et al. (2012) also mentioned that 12 DE starch couldretain more b-carotene, as compared to 6 DE starch, assaccharides with long chains are more permeable to oxygen.Microencapsulation of canthaxanthin produced by thebacterium Dietzia natronolimnaea HS-1 using differentconcentrations of soluble soybean polysaccharides by spraydrying (Hojjati et al. 2011) revealed that the degradation ofcanthaxanthin in the nonencapsulated samples was fasterthan that in the microencapsulated canthaxanthin samples.Another study performed by Santana et al. (2014) demon-strated that pequi pulp prepared with a modified starchconcentration of 22.5% had higher total carotenoids than thatprepared with a modified starch concentration of 27% and30%. Santana et al. (2014) revealed that high concentration ofmodified starch results in increased porosity, which mightinfluence the oxidative stability of carotenoids. Black pepperoleoresin was microencapsulated using gum Arabic and modi-fied starch by spray drying (Shaikh, Bhosale, and Singhal2006). According to Shaikh, Bhosale, and Singhal (2006), gumArabic was more capable of protecting oleoresin than modi-fied starch. Gum Arabic could restrain cracking of the matrixdue to good film-forming capability and plasticity (Shaikh,Bhosale, and Singhal 2006). Another study from Mahfoudhiand Hamdi (2015) evaluated that encapsulation with almondgum showed better protection of b-carotene against oxidationthan encapsulation with gum Arabic. Therefore, results frommany studies summarized that carrier agents are capable ofpreventing oxidation of carotenoids from oxygen, light, andtemperature. However, as every encapsulation material hasdifferent characteristics, selecting a suitable material is anessential step for encapsulation of carotenoids.

Encapsulations of carotenoids using protein

Encapsulations of carotenoids using protein are shown inTable 2. High content and lower degradation rate of

carotenoids were observed on encapsulation with gelatin,rather than starch because of protective power of gelatinagainst oxidative damage (Robert et al. 2003).Microencapsulation of b-carotene by soy protein isolatecould improve the storage stability of b-carotene as com-pared to the Microencapsulation of b-carotene by modifiedstarch (Deng et al. 2014). Similar results were also observedby Nogueira, Prestes, and de Medeiros Burkert (2017) whomentioned that soy protein might have ability to increasethe stability of carotenoids. Rasc�on et al. (2011) revealedthat carotenoid retention was higher in the microcapsulesprepared with soya protein than microcapsules preparedwith gum Arabic and they also mentioned that the yellowfraction was more stable than the red fraction due to differ-ences in their chemical structures. Zhao, Shen, and Guo(2018) showed whey protein could protect lutein contentfrom oxidation during storage.

Encapsulation of carotenoids using mixtures of variousencapsulation agents

Table 3 shows the encapsulation of carotenoids using mix-tures of maltodextrin and protein. Different ratios (1:9 to3:7) of gelatin to sucrose were used to prepare lycopenemicrocapsules from tomato paste during spray drying. Theresults showed that a gelatin to sucrose ratio of 3:7 wasgood for encapsulation, based on the encapsulation yieldand encapsulation efficiency (Shu et al. 2006). Theseresearchers also showed that the microencapsulated samplesshowed higher stability during storage, as compared withthe non-microencapsulated control because of oxidative sta-bility. Ranveer et al. (2015) showed that 90% lycopene fromtomato waste was retained in the microencapsulated samplesusing a gelatin to sucrose ratio of 3:7, whereas non encapsu-lated samples retained less than 5% lycopene during storage.Encapsulation of lycopene with gum Arabic and sucroseshowed that gum Arabic treated powder had good encapsu-lation efficiency during spray drying (Nunes andMercadante 2007). However, lycopene and b-cyclodextrin(1:4) mixture was more suitable for encapsulation, as com-pared to lycopene and b-cyclodextrin mixture (1:1), due tocomplex formation during freeze drying (Nunes and

Table 2. Encapsulation of carotenoids using proteins.

Sources of carotenoids Drying conditions Carrier agents Compounds References

Rosa Mosqueta(Rosa rubiginosa)

For starchInlet temperatures: 150 ± 5 �COutlet temperature: 70 ± 5 �CAtomization pressure: 3 kg/cm2

For gelatinInlet temperature: 100 ± 5 �COutlet temperature: 65 ± 5 �CAtomization pressure: 5 kg/cm2

gelatin and starch Trans-b-caroteneTrans-lycopeneTrans-rubixanthin

Robert et al. (2003)

Standard b-carotene Inlet temperature: 160Outlet temperature: 85 �C

soy protein isolate andOSA-modified starch

b-carotene Deng et al. (2014)

Phaffia rhodozyma Freeze drying soy protein carotenoid Nogueira, Prestes, and deMedeiros Burkert (2017)

Paprika (Capsicum annuum) Inlet temperature: 160 ± 5 �C,180 ± 5 �C, 200 ± 5 �C

Outlet temperature: 110 ± 5 �C

soy protein isolate andgum arabic

Yellow carotenoidRed carotenoid

Rasc�on et al. (2011)

Lutein – whey protein Lutein Zhao, Shen, and Guo (2018)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 7

Table 3. Encapsulation of carotenoids using mixture of maltodextrins and proteins.

Sources of carotenoids Drying conditions Carrier agents Compounds References

Tomato paste (Lycopersiconesculentum Mill.)

Inlet temperature: 170–210 �COutlet temperature: 35–65 �CAir flow rate: 2 m/sFeed flow rate: 100mL/h

Sucrose and gelatin (1:9, 2:8,3:7, 4:6, 5:5 w/v)

Lycopene Shu et al. (2006)

Tomato waste (Lycopersiconesculentum Mill.)

Inlet temperature: 160 �C,170 �C, 180 �C,

Outlet temperature: 35–65 �CAir flow rate: 2 m/sFeed flow rate: 2mL/min

Sucrose and gelatin (6:4, 7:3,and 8:2 w/v)

Lycopene Ranveer et al. (2015)

Tomato (Lycopersiconesculentum Mill.)

Inlet temperature: 170 ± 2 �COutlet temperature:113 ± 2 �CAir flow rate: 30mL/minAir pressure: 5 kgf/cm2

Gum arabic and sucrose (8:2) Lycopene Nunes and Mercadante (2007)

Tomato (Lycopersiconesculentum Mill.)

Freeze drying 1:1 and 1:4 (w/w) oflycopene and b cyclodextrin

Lycopene Nunes and Mercadante (2007)

Carrot pulp waste(Daucus carota L.)

Inlet temperature:135 �C–145 �C

Outlettemperature: 90–100 �C

35 g sucrose and 25 g gelatin All trans forms and cis formsof lutein, b-carotene,and a-carotene

Chen and Tang (1998)

Pink-grape fruit(Citrus paradise)

Freeze drying Alginate, sugars andgalactomannans

Lycopene Aguirre Calvo, Busch, andSantagapita (2016)

Annatto Spray drying Gum Arabic, Maltodextrinand Tween 80

Bixin Barbosa, Borsarelli, andMercadante (2005); DeMarcoa et al. (2013)

Annatto Spray drying Gum Arabic, Maltodextrinand Tween 80

Bixin Barbosa, Borsarelli, andMercadante (2005); DeMarcoa et al. (2013)

Paprika (Capsicum annuum) Inlet temperature: 170 ± 5 �COutlet temperature: 95 ± 5 �CAtomization pressure: 4.5 bar

Blend of 17% whey proteinconcentrate, 17% mesquitegum, and 66% (w/w)maltodextrin, or a blend of66% whey proteinconcentrate, 17% mesquitegum, and 17%maltodextrin (w/w) with awall to core material ratioof 2:1 and 4:1,respectively.

Oleoresin Perez-Alonso et al. (2008)

Red chilies (Capsicumannuum)

Inlet temperature: 170 ± 5 �COutlet temperature: 80 ± 5 �CAir pressure: 2.8 barFeed flow rate: 20mL/min

Gellan gum, 10 DEmaltodextrin,

mesquite gum

Carotenoid Rodriguez-Huezo et al. (2004)

Chili pepper (Capsicumannuum)

Inlet temperature: 160 ± 2 �COutlet temperature: 70 ± 2 �CAir pressure: 0.4 kg/cm2

Feed flow rate: 13.3mL/min

Gum arabic and maltodextrin Carotenoids Guadarrama-Lezamaet al. (2012)

Cumin Inlet temperature: 160 ± 2 �COut temperature: 120 ± 5 �CFlow rate: 300 g/h.

Gum arabic, maltodextrin,and modified starch

oleoresin Kanakdande, Bhosale, andSinghal (2007)

Dunaliella salina Inlet temperature: 200 �C,265 �C

Outlet temperature: 100 �C,120 �CAir pressure: 0.4 kg/cm2

Feed flow rate: 13.3mL/min

12 DE maltodextrin and gumarabic at a ratio of 3.5:1

b-carotene Leach, Oliveira, andMorais (1998)

Brown seaweed(Phaeophyceae)

Freeze drying at �45 �Cunder high (0.04 mbar)vacuum conditions.

maltodextrin (70.02 g) andTween 80 (1.07 g)

Fucoxanthin Indrawati et al. (2015)

Lutein crystals Inlet air temperature,185 ± 1 �C; Outlet airtemperature, 85 ± 1 �C

Ratio of maltodextrin-sucrose(3:0, 3:1 and 3:3)

Lutein Kuang et al. (2015)

Gac fruit (Momordicacochinchinensis)

Inlet temperature: 154 �COutlet temperature: 80 �CFeed flow rate: 970mL/h,Air flow speed: 4.3 m/sPressure: 2 bar

Whey protein concentrateand gum arabic (7:3 g/g)

b-carotene and lycopene Kha et al. (2015)

Neurospora Inlet temperature: 170 �C,180 �C

Outlet temperature: 60 �C,70 �C

Feed flow rate: 8mL/min

Different concentrations (20%,30%, and 40% w/w) ofsodium caseinate, soyprotein isolate, and wheyprotein isolate

Total carotene Pahlevi, Estiasih, andSaparianti (2008)

(continued)

8 J.-B. EUN ET AL.

Mercadante 2007). Carotenoid powder from carrot pulpwaste was processed with sucrose and gelatin by spray dry-ing (Chen and Tang 1998). The study reported that the deg-radation of all-trans-lutein was lower than those ofa-carotene and b-carotene, due to the formation of lutein-gelatin complexes during spray drying. Lycopene was encap-sulated with alginate along with sugars and galactomannansfrom pink-grape fruit by freeze drying (Aguirre Calvo,Busch, and Santagapita 2016). Aguirre Calvo, Busch, andSantagapita (2016) showed that among different encapsulatingagents, alginate with trehalose and vinal gum could preservemore lycopene content due to minimized isomerization andstructural changes. Bixin was encapsulated using gum Arabicand maltodextrin with sucrose and Tween 80 from annattoseeds by spray drying (Barbosa, Borsarelli, and Mercadante2005; De Marcoa et al. 2013). The authors observed that bixinencapsulated with gum Arabic, rather than maltodextrin, pro-vided better protection against oxidation and photochemicaldegradation. Red chili oleoresin was microencapsulated with ablend of 17% whey protein concentrate, 17% mesquite gum,and 66% (w/w) maltodextrin, or a blend of 66% whey proteinconcentrate, 17% mesquite gum, and 17% maltodextrin (w/w)with a wall to core material ratio of 2:1 and 4:1, respectively(Perez-Alonso et al. 2008).The results from this study showedthat the higher wall-to-core ratio (4:1) provided maximumprotection against oxidation. Rodriguez-Huezo et al. (2004)observed that a higher wall-to-core material ratio could helpin retaining higher amounts of carotenoids in red chili.Guadarrama-Lezamaetet al. (2012) microencapsulated carote-noids from non-aqueous extracts of chili pepper by usingthree different oils (corn, sunflower, and safflower), as well asgum Arabic and maltodextrin in a ratio of 4:1 (w/w), as wallmaterials. They found that carotenoid degradation was lowerin the microencapsulated samples than in the non micro-encapsulated samples because microencapsulation protectsagainst both oxidation and degradation (Guadarrama-Lezamaetet al., 2012). Cumin oleoresin microencapsulationwas performed using a combination of gum Arabic, maltodex-trin, and modified starch (Kanakdande, Bhosale, and Singhal2007). The results showed that gum Arabic blendedwith maltodextrin and modified starch at a ratio of 4/6, 1/6,and 1/6 could better prevent oxidation of oleoresin, as com-pared to other encapsulating agents. Encapsulated powders ofDunaliella salina were prepared using maltodextrin and gumArabic by spray drying. The b-carotene in powders treatedwith maltodextrin and gum Arabic was more stable, as com-pared to the control. The storage stability of the encapsulatedpowders also increased significantly (Leach, Oliveira, andMorais 1998). The carrier agents could possibly retard the

oxygen diffusion, thus contributing to the stabilization ofb-carotene in encapsulated powders. The encapsulated pig-ment prepared from brown seaweed (Sargassum spp.) usingfreeze drying with maltodextrin and Tween-80 as encapsulat-ing agents showed that carotenoids from the brown seaweedcould be extracted using encapsulating agents (Indrawati et al.2015) and that carrier agents could act as barriers of auto-oxida-tion. Lutein crystal was microcapsulated with maltodextrins andsucrose by spray drying (Kuang et al. 2015), showed oxidationresistance due to the carrier agents. Kha et al. (2015) also foundwhey protein and gum Arabic could be retained more b-carotenedue to protective effect of carotenoid from oxidation during spraydrying. Pahlevi, Estiasih, and Saparianti (2008) extracted carotenefrom Neurospora using different concentrations (20%, 30%, and40% w/w) of sodium caseinate, soy protein isolate, and whey pro-tein isolate through spray drying. The results showed that encap-sulation with 30% sodium caseinate resulted in maximum totalcarotenoid content. Pahlevi, Estiasih, and Saparianti (2008) dem-onstrated that sodium caseinate could form a double layer, thusresulting in better resistance to oxidation, as compared to the pro-tein isolate. Lam Dien, Minh, and Anh Dao (2013) showed thatcarotene loss in gac fruit could be prevented using maltodextrinand gelatin. Neurospora intermedia N-1 was used to extract caro-tenoids with gelatin-maltodextrins using spray drying (Gusdinaret al. 2011).The results showed that the encapsulated powderswere more stable than the non-encapsulated powder.

Factors affecting stability of encapsulatedcarotenoids

Various conditions, such as relative humidity (RH), tem-perature, light, and heat play significant roles in retention ofcarotenoids during storage. Mahfoudhi and Hamdi (2015)reported that lower RH (10%) during storage showed lowerdegradation rate of encapsulated trans b-carotene with gumArabic and almond gum, as compared to higher RH (45 and80%). Similar trends were shown by Sutter, Buera, andElizalde (2007), who encapsulated trans b-carotene usingmannitol by freeze drying and Deng et al. (2014) encapsu-lated b-carotene using soy protein isolate and octenylsuc-cinic anhydride-modified starch by spray drying. Moststudies reported that initially, the content of encapsulatedcarotenoids decreased very fast, followed by slower decreaseat lower RH (up to 75%) during storage. However, Sutter,Buera, and Elizalde (2007) showed that encapsulated b-caro-tene content sharply reduced in the first stage, thendecreased constantly, and finally showed a sudden decrease.Different RH values showed different retention values ofb-carotene due to oxidative stability. However, storage at

Table 3. Continued.

Sources of carotenoids Drying conditions Carrier agents Compounds References

Gac fruit (Momordicacochinchinensis Spreng)

– Ratio of maltodextrin-gelatin(10%, 20%, 30%, 40%, and50% w/v)

Total carotenoid content Lam Dien, Minh, and AnhDao (2013)

Neurospora intermedia N-1 Inlet temperature: 160 �COutlet temperature: 70 �CAir pressure: 1 barFeed flow rate: 8mL/min

13–17 DE maltodextrin andgelatin at a ratio of 4:1

Carotenoids Gusdinar et al. (2011)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 9

higher RH (75% or above) revealed greater reduction inb-carotene content, possibly related to structure collapse.Collapse of structure is related to oxygen diffusion fromsurface to matrix, and thus to the decrease in the retention ofb-carotene. Particle size and surface carotene could influencethe retention of b-carotene (Sutter, Buera, and Elizalde 2007).Kha et al. (2015) encapsulated gac oil powder with whey pro-tein concentrate and gum Arabic. Their results revealed thatencapsulated powder of b-carotene and lycopene should notbe kept at higher equilibrium relative humidity (75%), as thehigher moisture content results in more chemical, biological,and microbial degradation during the storage period.Moreover, Desobry, Netto, and Labuza (1999) did not findany significant differences between 11% and 33% RH forb-carotene encapsulated with two maltodextrins, 15 DE and 4DE. Similar results were shown by Desobry, Netto, andLabuza (1997) for pure b-carotene using maltodextrin DE 25by spray and freeze drying. However, Qv, Zeng, and Jiang(2011) demonstrated that lower relative humidity (33%)showed higher retention (90.16%) of lutein microcapsulewith gelatin and gum Arabic, whereas 68.18% and 30.15%retention was observed for lutein at higher relative humidity(80%) and non-encapsulated lutein, respectively.

Conditions of higher temperature and light exposureduring storage were more destructive than lower tempera-ture and dark conditions for encapsulated all trans b-caro-tene, all trans a-carotene, and all trans-lutein of carotenoidpowders from carrot pulp using sucrose and gelatin thoughspray drying, due to increased occurrence of isomerization(Chen and Tang 1998). The results also showed thatall trans b-carotene was more susceptible to degradationthan all trans a-carotene and all trans-lutein during variousstorage conditions. Similar phenomena were observed byChiu et al. (2007) for the encapsulation of cis-trans-andtotal lycopene from tomato pulp waste using gelatin andpolyglutamic acid by freeze drying. However, light did notaccelerate the degradation rates of encapsulated b- caroteneand a-carotene using various carrier agents from carrot(Wagner and Warthesen 1995). However, light and highertemperature also reduced the retention of lutein in microen-capsulated with gelatin and gum Arabic due to loss of glassstate, as well as increase in the molecular chain (Qv, Zeng,and Jiang 2011). Rasc�on et al. (2011) observed increase incarotenoids with increasing inlet air temperature in encapsu-lated using gum Arabic and soy protein isolate from paprikaoleoresin, due to higher yield and retention of volatilecompounds. Encapsulated bixin using gum Arabic or malto-dextrin was more stable than non-encapsulated bixin, andalso showed greater stability in dark conditions than inlight condition throughout storage (Barbosa, Borsarelli,and Mercadante 2005). The authors reported protectionagainst photodegradation, as well as occurrence of isomers,under light conditions, thus influencing the retention of bixin.Encapsulated curcumin with maltodextrin, modified starch, andgum Arabic showed higher retention, followed by encapsulationwith gum Arabic and combination of maltodextrin and modifiedstarch for spray drying during storage under light (Cano-Higuita,Malacrida, and Telis 2015). Combination of maltodextrin,

modified starch, and gum Arabic could prevent curcumin lossdue to oxidation. However, using freeze drying, encapsulated cur-cumin from turmeric with gum Arabic retained higher levels ofcurcumin, as compared to curcumin encapsulated with ternarymixture (maltodextrin, modified starch, and gum Arabic) andbinary mixture (maltodextrin and starch) during storage underlight (Cano-Higuita, Malacrida, and Telis 2015). Encapsulatedcanthaxanthin showed greater stability in dark conditions thanexposed to light (Hojjati et al. 2011). Similar behavior was foundby Ranveer et al. (2015), who also reported that encapsulation oflycopene with sucrose and gelatin in refrigerated temperature andabsence of light showed higher retention of lycopene than that atroom temperature and in the presence of light. Therefore, lowerstorage temperature, relative humidity below 75%, and darkconditions would be the ideal conditions for maximum retentionof carotenoids during storage.

Relationship between coating materials andmicrostructure on encapsulated carotenoids

Retention of carotenoids is influenced by the microstructureof the encapsulating material. Morphological structures ofmicrocapsules are also affected by different wall materials.Microstructure of cumin oleoresin microencapsulated withgum Arabic was smooth and irregular, as well as shrinkageof the particle and cavity form, which could result in moreprotection of cumin than microencapsulation with malto-dextrin and modified starch (Kanakdande, Bhosale, andSinghal 2007) (Figure 8). Similar structure was also observedfor bixin encapsulated with gum Arabic and sucrose, whilethat of bixin encapsulated with maltodextrin and sucrose ormaltodextrin and Tween was different (Barbosa, Borsarelli,and Mercadante (2005) (Figure 9). Microencapsulation withgum Arabic, maltodextrin, and modified starch showedhigher retention of cumin oleoresin due to more uniformand less cracked structure, as compared to the micro-encapsulation with maltodextrin, modified starch, and gumArabic (Kanakdande, Bhosale, and Singhal 2007) (Figure 8).Microencapsulated lycopene with gelatin and sucroseshowed a bee-hive like structure, whereas non-encapsulatedlycopene showed saw dust like structure. Bee -hive resem-bling structure might be related to the evaporation rate ofwater from core of microencapsulation that could influencethe retention of lycopene during storage (Figure 10). Theaforementioned discussion indicates that the carotenoidscontent depends on microstructure, as well as carrier agents.

Effects of glass transition temperature (Tg) onencapsulated carotenoids

Usually structure collapse, shrinkage, and caking occur abovethe glass transition temperature (Tg) (Coronel-Aguilera andMartin-Gonzalez 2015). Tg also is related to oxygen transfer(Desobry, Netto, and Labuza 1999). Some studies foundhigher b-carotene losses in the glassy state (below Tg) (Prado,Buera, and Elizalde 2006). Encapsulated of b-carotene withmaltodextrin showed lower rate of b-carotene loss than thatencapsulated with a mixture of maltodextrin and gum Arabic

10 J.-B. EUN ET AL.

and with a mixture of maltodextrin and gelatin, due to higherglassy state (Ramoneda et al. 2011). These studies alsorevealed that the maximum b-carotene degradation wasobserved when the Tg value was lower than the storagetemperature. However, Desobry, Netto, and Labuza (1999)did not observe these phenomena on encapsulation of transb-carotene with glucose, galactose, and lactose, along withtwo maltodextrins: 15 DE and 4 DE. Their results showed theglassy state of encapsulated trans b-carotene on storage at atemperature below Tg, but it was not correlated with b-caro-tene retention. Therefore, the relation between glass transitiontemperature and encapsulated carotenoids remains unclear.

Degradation kinetics for encapsulated carotenoids

Modeling is used as powerful tool to predict the optimumstorage conditions for encapsulated carotenoids. Most of theencapsulated carotenoids models were described by first-order reaction, but some studies also dealt with zero-orderreactions throughout the storage period. Tables 4 and 5show the modeling of encapsulated carotenoids using sprayand freeze drying, respectively, during storage. Degradation

kinetics, such as degradation reaction rate, reaction order,rate constant, half-life, and activation energy are crucialparameters to know the storage conditions for shelf life ofencapsulated carotenoids. In this section, we elaborate thedegradation kinetics for encapsulated carotenoids using twoways: spray drying and freeze drying.

Modeling during spray drying

Most of authors used the Arrhenius model, but other mod-els such as the Weibull model, Kohlrausch–Williams–Wattsmodel, and Regression model were also used by few authors.Reaction rate constant, half-life, and activation energydepend on the sources of carotenoids, carrier agents, storagetemperature, and storage conditions (Table 4). Higherdegradation rate and lower half-life were found with increas-ing storage temperature for all encapsulated carotenoids.Encapsulated lycopene showed a higher degradation ratethan encapsulated b-carotene (Kha et al. 2015). Theseauthors also reported that encapsulated carotenoids withgelatin showed higher activation energies, as comparedwith those encapsulated with starch. Degradation rate and

Figure 8. Microcapsules prepared from gum arabic (a), maltodextrin (b), modified starch (c), d) gum arabic/maltodextrin/modified starch(4/6:1/6:1/6) (adapted fromKanakdande, Bhosale, and Singhal 2007).

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 11

activation energy might be related to the various complexstructures and reactivities of carotenoids connecting withthe matrix of encapsulating materials during storage.Carotenoids and surrounding matrix interactions could alsoinfluence the degradation rate and activation energy (Khaet al. 2015). Most of the encapsulated carotenoid modelswere described by first-order reactions, but some studiesalso dealt with other reaction models throughout the storage

period. Non-encapsulated bixin showed a single first-orderdecay, whereas encapsulated bixin showed two sequentialfirst-order decays under dark condition because moreoxidative and photochemical degradation occurred inthe non-encapsulated sample (Barbosa, Borsarelli, andMercadante 2005). However, Kuang et al. (2015) found thatthe Kohlrausch–Williams–Watts model was a good fit forencapsulated lutein. Thus, various models might be used to

Figure 9. SEM micrographs of spray-dried microencapsulated bixin with (a) GA/sucrose (95:5), (b) MD 20 DE/sucrose (80:20), (c) 100% MD 20 DE (d) MD 20 DE/Tween 80 (99.8:0.2). The magnification of all micrographs was 1400 (adapted from Barbosa, Borsarelli, and Mercadante 2005).

Figure 10. (A) Lycopene without encapsulation and (B) microencapsulated lycopene (adapted from Ranveer et al. 2015).

12 J.-B. EUN ET AL.

Table4.

Degradatio

nkineticsmod

elingof

encapsulated

caroteno

idsdu

ringspraydrying

.

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Rosa

Mosqu

eta

(Rosarubiginosa)

Storageat

(55,

40,

and25

� C)

Starch

andgelatin

First-orderkinetic

mod

el.

lnC¼lnC o–k(t)

Arrheniusmod

elk¼Ae

�(Ea/R)/T

ForStarch

trans-b-Carotene

K 25�C¼6.7�10

�3±5�10

�4(h

�1)

K 40�C¼2.5�10

�2±3�10

�3(h

�1)

K 55�C¼5.1�10

�2±5�10

�3(h

�1)

t 1/2

(21�C)¼

5(days);Ea¼13.1±1.5(Kcal/m

ol)

trans-Lycopene

K 25�C¼7.5�10

�3±8�10

�4(h

�1)

K 40�C¼2.2�10

�2±3�10

�3(h

�1)

K 55�C¼4.0�10

�2±6�10

�3(h

�1)

t 1/2

(21�C)¼

5(days);Ea¼10.9±1.1(Kcal/m

ol)

trans-Ru

bixanthin

K 25�C¼8.0�10

�3±9�10

�4(h

�1)

K 40�C¼2.9�10

�2±4�10

�3(h

�1)

K 55�C¼6.4�10

�2±1�10

�2(h

�1)

t 1/2

(21�C)¼

5(days);Ea¼13.4±1.1(Kcal/m

ol)

ForGelatin

trans-b-Carotene

K 25�C¼1.9�10

�3±1�10

�4(h

�1)

K 40�C¼9.5�10

�3±1�10

�3(h

�1)

K 55�C¼3.7�10

�2±4�10

�3(h

�1)

t 1/2

(21�C)¼

23(days)Ea

¼19.2±0.1(Kcal/m

ol)

trans-Lycopene

K 25�C¼4.6�10

�3±6�10

�4(h

�1)

K 40�C¼1.5�10

�2±1�10

�3(h

�1)

K 55�C¼4.1�10

�2±5�10

�3(h

�1)

t 1/2

(21�C)¼

9(days)Ea

¼14.2±0.2(Kcal/m

ol)

trans-Ru

bixanthin

K 25�C¼3.2�10

�3±3�10

�4(h

�1)

K 40�C¼1.8�10

�2±3�10

�3(h

�1)

K 55�C¼3.4�10

�2±5�10

�3(h

�1)

t 1/2

(21�C)¼

11(days)Ea

¼15.4±3.5(Kcal/m

ol)

Robertet

al.(2003)

Carrot

Storageat

(21�C)

Dry

hydrolyzed

starch

(4DE,‘

15DE,25DEor

36.5DE)

First-orderkinetic

mod

el.

t 1/2¼0.693/k

Arrheniusmod

elk¼K 0e�

(Ea/R)/T

Formajor

carotenes

a-Carotene

K 4DE¼8.39xl09.e�9.23x103/T

(h�1 );t

1/2¼

149(days)

K 15D

E¼1.01xl09.e�8.77x103/T

(h�1);t 1/2¼

258(days)

K 25D

E¼4.41xl01

0 .e�

9.82x103/T

(h�1);t 1/2¼

210(days)

K 36.5D

E¼2.18xl01

1 .e�

1.05x104/T

(h�1);t 1/2¼

458(days)

b-Carotene

K 4DE¼5.35xl09.e�9.09x103/T

(h�1 );t

1/2¼

145(days)

K 15D

E¼3.93xl08.e�8.47x103/T

(h�1);t 1/2¼

237(days)

K 25D

E¼4.03xl01

0 .e�

9.79x103/T

(h�1);t 1/2¼

209(days)

K 36.5D

E¼1.18xl01

1 .e�

1.03x104/T

(h�1);t 1/2¼

431(days)

Forsurfacecarotene

a-Carotene

10%

K 15D

E¼1.82

±0.258x10�

2(day

�1 )

15%

K 15D

E¼1.66

±0.215x10�

2(day

�1 )

20%

K 15D

E¼0.896±0.144x10�

2(day

�1 )

25%

K 15D

E¼0.451±0.107x10�

2(day

�1 )

b-Carotene

10%

K 15D

E¼1.82

±0.260x10�

2(day

�1 )

Wagnerand

Warthesen

(1995)

(continued)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 13

Table4.

Continued.

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

15%

K 15D

E¼1.65

±0.219x10�

2(day

�1 )

20%

K 15D

E¼0.908±0.153x10�

2(day

�1 )

25%

K 15D

E¼0.493±0.129x10�

2(day

�1 )

Dunaliella

salina

Storageat

(room

temperature)

12DEmaltodextrin

andgu

marabicat

aratio

of3.5:1

First-orderkinetic

mod

el.

b-Carotene

Inlettemperature

for200�C

K¼0.06

(day

�1)

Inlettemperature

for265�C

K¼0.10

(day

�1)

Leach,

Oliveira,and

Morais(1998)

Gac

(Mom

ordica

cochinchinensis)

Storageat

(�20

� C,

10� C

androom

temperature

(25–30

� C)for

360

days,at40

� Cfor

120days

andat

63� C

for28

days.

wheyprotein

concentrateandgu

mArabic

First-orderkinetic

mod

el.

lnC¼ln

C0–kt

t 1/2¼ln

2/k.

Arrheniusmod

el

k¼Ae

�Ea/RT

b-Carotene

K Vacuumþdarkat

�20�C¼0.0002

(day

�1 );t

1/2¼3466

(days)

K Non

-vacuumþdark�20

� C¼0.0003

(day

�1);t 1/2¼2310

(days)

k Vacuumþdarkat

10� C¼0.0004

(day

�1 );t

1/2¼1733

(days)

K Non

-vacuumþdarkat

10� C¼0.0009

(day

�1 );t

1/2¼770(days)

K Vacuumþdarkat

RT¼0.0005

(day

�1 );t

1/2¼1386

(days)

K Non

-vacuumþdarkat

RT¼0.0013

(day

�1 );t

1/2¼533(days)

K Vacuumþlightat

RT¼0.0009

(day

�1 );t

1/2¼770(days)

K Non

-vacuumþlightat

RT¼0.0015

(day

�1);t 1/2¼462(days)

K Vacuumþdarkat

40� C¼0.0038

(day

�1);t 1/2¼182(days)

K Non

-vacuumþdarkat

40� C¼0.0063

(day

�1 );t

1/2¼110(days)

K Vacuumþdarkat

63� C¼0.0062

(day

�1);t 1/2¼10

(days)

K Non

-vacuumþdarkat

63� C¼0.1018

(day

�1 );t

1/2¼7(days)

Lycopene

K Vacuumþdarkat

�20�C¼0.0004

(day

�1 );t

1/2¼1733

(days)

K Non

-vacuumþdark�20

� C¼0.0004

(day

�1);t 1/2¼1733

(days)

k Vacuumþdarkat

10� C¼0.0004

(day

�1 );t

1/2¼1733

(days)

K Non

-vacuumþdarkat

10� C¼0.0006

(day

�1 );t

1/2¼1155

(days)

K Vacuumþdarkat

RT¼0.0011

(day

�1 );t

1/2¼630(days)

K Non

-vacuumþdarkat

RT¼0.0020

(day

�1 );t

1/2¼347(days)

K Vacuumþlightat

RT¼0.0012

(day

�1 );t

1/2¼578(days)

K Non

-vacuumþlightat

RT¼0.0022

(day

�1);t 1/2¼315(days)

K Vacuumþdarkat

40� C¼0.0048

(day

�1);t 1/2¼144(days)

K Non

-vacuumþdarkat

40� C¼0.0077

(day

�1 );t

1/2¼90

(days)

K Vacuumþdarkat

63� C¼0.0748

(day

�1);t 1/2¼9(days)

K Non

-vacuumþdarkat

63� C¼0.1265

(day

�1 );t

1/2¼5(days)

Khaet

al.(2015)

Blackpepp

erStorageat

31� C

for

6weeks.

Gum

arabicand

mod

ified

starch

First-orderkinetic

mod

el.

t 1/2¼0.693/k

Oleoresin

ForEntrappedpiperin

et (1

/2)gum

arabic¼71.44(weeks)

t (1/2)mod

ified

starch¼55

(weeks)

ForTotalp

iperine

t (1/2)gum

Arabic¼121.57

(weeks)

t (1/2)mod

ified

starch¼128.33

(weeks)

Fortotalvolatiles

t (1/2)gum

Arabic¼25.76(weeks)

t (1/2)mod

ified

starch¼26.34(weeks)

Forno

n-volatiles

t (1/2)gum

Arabic¼77.86(weeks)

t (1/2)mod

ified

starch¼41.49(weeks)

Shaikh,B

hosale,

and

Sing

hal(2006)

Redchilies

Storageat

31� C

for

35days

Gellangu

m,1

0DE

maltodextrin

,mesqu

itegu

m

zero-order

degradation

reactio

nt (1

/2)¼0.5/K

Caroteno

ids

K(x¼35%,y

¼3.9)¼0.0235

(day

�1);t (1

/2)¼21.3

(days)

K(x¼25%,y

¼3.9)¼0.0242

(day

�1);t (1

/2)¼20.7

(days)

K(x¼35%,y

¼2.6)¼0.0271

(day

�1);t (1

/2)¼18.4

(days)

K(x¼25%,y

¼2.6)¼0.0234

(day

�1);t (1

/2)¼21.4

(days)

K(x¼35%,y

¼1.4)¼0.0236

(day

�1);t (1

/2)¼21.2

(days)

K(x¼35%,y

¼1.4)¼0.0200

(day

�1);t (1

/2)¼25.0

(days)

Rodriguez-Huezo

etal.(2004)

(continued)

14 J.-B. EUN ET AL.

Table4.

Continued.

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Paprika

Storageat

31� C

with

diffe

rent

a wfor35

days

gum

ArabicandSoyprotein

isolate(SPI)

First-orderkinetic

mod

el.

Redfractio

noleoresin

K v(0.108)gum

arabic¼33.09±0.93

x10�

3(day

�1 )

K v(0.318)gum

arabic¼55.73±0.63

x10�

3(day

�1 )

K v(0.515)gum

arabic¼123.89

±1.88

x10�

3(day

�1 )

K v(0.743)gum

arabic¼31.60±3.15

x10�

3(day

�1 )

K v(0.108)SPI¼

197.95

±10.94x10�

3(day

�1)

K v(0.318)SPI¼

201.32

±2.88

x10�

3(day

�1)

K v(0.515)SPI¼

196.45

±6.18

x10�

3(day

�1)

K v(0.743)SPI¼

40.15±1.94

x10�

3(day

�1)

Yellow

fractio

noleoresin

K v(0.108)gum

arabic¼37.33±1.52

x10�

3(day

�1 )

K v(0.318)gum

arabic¼55.41±0.75

x10�

3(day

�1 )

K v(0.515)gum

arabic¼130.17

±3.98

x10�

3(day

�1 )

K v(0.743)gum

arabic¼31.60±3.15

x10�

3(day

�1 )

K v(0.108)SPI¼

190.3±7.02

x10�

3(day

�1)

K v(0.318)SPI¼

209.75

±2.25

x10�

3(day

�1)

K v(0.515)SPI¼

217.81

±11.64x10�

3(day

�1)

K v(0.743)SPI¼

38.55±1.08

x10�

3(day

�1)

Rasc� on

etal.(2011)

Turm

eric

Storageat

25� C

for

4weeks

gum

arabicmaltodextrin

mod

ified

starch

pseudo

-firstorderkinetics.

Regression

mod

elCu

rcum

inMaltodextrin

(75%

)andmod

ified

starch

(25%

)ln(CR)¼4.67

-0.193(t)

Gum

arabic

ln(CR)¼4.48

-0.094(t)

gum

Arabic(33%

),maltodextrin

(33%

)andmod

ified

starch

(33%

)ln(CR)¼4.63

-0.043(t)

Cano

-Higuita,

Malacrid

a,and

Telis

(2015)

Cumin

Storageat

25� C

for

6weeks

Gum

arabic;M

odified

starch;

Maltodextrin

First-orderkinetic

mod

el.

t 1/2¼0.693/k

Oleoresin

Totalcum

inaldehyde

t (1/2)gum

arabic¼57.75(weeks)

t (1/2)m

odified

starch¼14.71(weeks)

t (1/2)m

altodextrin¼22.28(weeks)

Totalc-terpinene

t (1/2)gum

arabic¼30.13(weeks)

t (1/2)m

odified

starch¼12.92(weeks)

t (1/2)m

altodextrin¼6.86

(weeks)

Totalp

-cym

ene

t (1/2)gum

arabic¼45.0

(weeks)

t (1/2)m

odified

starch¼22.35(weeks)

t (1/2)m

altodextrin¼36.28(weeks)

Totalv

olatiles

t (1/2)gum

arabic¼50.58(weeks)

t (1/2)m

odified

starch¼9.57

(weeks)

t (1/2)m

altodextrin¼28.75(weeks)

Kanakdande,

Bhosale,and

Sing

hal(2007)

Cumin

Storageat

25� C

for

6weeks

Differentconcentrationof

gum

Arabic;m

odified

starch

andmaltodextrin

First-orderkinetic

mod

el.

t 1/2¼0.693/k

Totalcum

inaldehyde

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/3,1/3,1/3)¼27.60(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(4/6,1/6,1/6)¼55.88(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,4/6,1/6)¼16.11(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,1/6,4/6)¼19.63(weeks)

Totalc-terpinene

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/3,1/3,1/3)¼9.88

(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(4/6,1/6,1/6)¼35.53(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,4/6,1/6)¼9.07

(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,1/6,4/6)¼11.12(weeks)

Kanakdande,

Bhosale,and

Sing

hal(2007)

(continued)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 15

Table4.

Continued.

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Totalp

-cym

ene

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/3,1/3,1/3)¼22.72(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(4/6,1/6,1/6)¼60.78(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,4/6,1/6)¼15.82(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,1/6,4/6)¼27.07(weeks)

Totalv

olatiles

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/3,1/3,1/3)¼28.87(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(4/6,1/6,1/6)¼85.55(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,4/6,1/6)¼34.13(weeks)

t (1/2)gum

arabic;mod

ified

starch;maltodextrin

(1/6,1/6,4/6)¼25.01(weeks)

Bixinfrom

annattoseed

Storageat

25� C

for

18days

under

light

and

dark

cond

ition

.

Arabicgu

mandmaltodextrin

DE10.

First-orderandsecond

-orderkinetic

mod

el.

t 1/2¼ln2/k

Arrheniusmod

elK (light)¼15.7�10

3(days�1 )t (1

/2)light¼44.15(days)

K (dark)¼3.0�10

3(days�1 )t (1

/2)light¼231.05

(days)

DeMarcoa

etal.(2013)

Bixinfrom

annattoseed

Storageat

21� C

for

400hun

der

light

and

dark

cond

ition

.

Arabicgu

m,m

altodextrin

DE

20andsucrose.

Photod

egradatio

nkinetics

[Bix] t¼[Bix] 0exp(-t/s i)

s F(95%

AGþ5%

SUC)¼

3.3(h),s s

(95%

AGþ5%

SUC)¼

66(h)

t S(95%

AGþ5%

SUC)¼

74(h),s D

(95%

AGþ5%

SUC)¼

12000(h)

s F(80%

MDþ20%

SUC)¼

3.5(h),s s

(80%

MDþ20%

SUC)¼

47(h)

t S(80%

MDþ20%

SUC)¼

27(h),s D

(80%

MDþ20%

SUC)¼

1400

(h)

s F(100%

MDþ0%

SUC)¼

1.2(h),s s

(100%

MDþ0%

SUC)¼

30(h)

t S(100%

MDþ0%

SUC)¼

27(h),s D

(100%

MDþ0%

SUC)¼

2700

(h)

s F(99.8%

MDþ0.2%

Tween80)¼

3.4(h),s s

(99.8%

MDþ0.2%

Tween80)¼

81(h)

t S(99.8%

MDþ0.2%

Tween80)¼

4(h),s D

(99.8%

MDþ0.2%

Tween)¼

2800

(h)

Barbosa,Bo

rsarelli,

and

Mercadante

(2005).

Pure

transb-carotene

Storageat

25� C

for

seventeenweeks

Maltodextrin

25DE

First-orderandsecond

-orderkinetic

mod

el.

Arrheniusmod

elK 2

5DE(t<

t c)¼

0.097±0.008,

E a¼14.19(Kcal/m

ol),t (1

/2)¼

7.1(weeks)

K 25D

E(t>

t c)¼

0.026±0.004,

E a¼7.69

(Kcal/m

ol),t (1

/2)¼

27.0

(weeks)

Desob

ry,N

etto,and

Labu

za(1997).

Lutein

crystals

Agingun

der5,

10and15

� CMaltodextrin

DE6.1

Kohlrausch–

Williams–Watts

(KWW)mod

el/t¼exp(–

t/s)

b

/t¼1-DHrelax/

DH1¼exp(–

t/s)

b

DH1

¼DCp

(Tg-Ta)

DH1

(5� C)¼

1.31

(J/g),s¼60.5

(h),b¼0.81

DH1

(10�C)¼2.00

(J/g),s¼161(h),b¼0.76

DH1

(15�C)¼3.93

(J/g),s¼316(h),b¼0.95

Kuanget

al.(2015)

Pure

b-carotene

Storageat

25� C

for

thirtydays

under

diffe

rent

relativehu

midity

Vario

usmod

ified

starches

such

as(OSA

1),(OSA

2)and

(OSA

3)

Time-course

degradationmod

elWeibu

llmod

elR¼exp[(kt)n]

OSA

1K (11%)¼

13.36±0.50

(10�

3 /day),O

SA1n (11%)¼

1.26

±0.040

OSA

1K (33%)¼

14.16±0.87

(10�

3 /day),O

SA1n (33%)¼

1.158±0.063

OSA

1K (52%)¼

33.92±0.50

(10�

3 /day),O

SA1n (52%)¼

1.478±0.060

OSA

1K (75%)¼

24.90±0.65

(10�

3 /day),O

SA1n (75%)¼

1.362±0.060

OSA

1K (97%)¼

18.36±0.51

(10�

3 /day),O

SA1n (97%)¼

0.997±0.024

OSA

2K (11%)¼

34.40±0.23

(10�

3 /day),O

SA2n (11%)¼

1.230±0.020

OSA

2K (33%)¼

38.92±0.37

(10�

3 /day),O

SA2n (33%)¼

1.243±0.028

OSA

2K (52%)¼

40.97±0.25

(10�

3 /day),O

SA2n (52%)¼

1.204±0.017

OSA

2K (75%)¼

44.06±0.98

(10�

3 /day),O

SA2n (75%)¼

1.222±0.063

OSA

2K (97%)¼

21.26±0.71

(10�

3 /day),O

SA2n (97%)¼

0.812±0.031

OSA

3K (11%)¼

33.2±0.42

(10�

3 /day),O

SA3n (11%)¼

1.237±0.036

OSA

3K (33%)¼

35.4±0.84

(10�

3 /day),O

SA3n (33%)¼

1.330±0.065

OSA

3K (52%)¼

38.44±0.83

(10�

3 /day),O

SA3n (52%)¼

1.300±0.062

OSA

3K (75%)¼

41.60±0.73

(10�

3 /day),O

SA3n (75%)¼

1.197±0.047

OSA

3K (97%)¼

19.94±0.38

(10�

3 /day),O

SA3n (75%)¼

1.009±0.022

Lianget

al.(2013).

Pure

transb-carotene

Storageat

25� C

for

17weeks

Vario

usconcentrations

ofglucose,

galactoseand

lactosewith

15DEand4

First-orderandsecond

-orderkinetic

mod

el.

Arrheniusmod

elb-Carotene

K 25D

E(t<

t c)¼

0.097,

E a¼14.187

(Kcal/m

ol),t (1

/2)¼

7.1±1.4(weeks)

K 25D

E(t>

t c)¼

0.026,

E a¼7.69

(Kcal/m

ol),t (1

/2)¼

27.0±2.5(weeks)

K 15G

lc(t<

t c)¼

0.126,

E a¼11.31(Kcal/m

ol),t (1

/2)¼

5.5±0.8(weeks)

Desob

ry,N

etto,and

Labu

za(1999).

(continued)

16 J.-B. EUN ET AL.

determine the shelf life of carotenoids encapsulated usingspray drying.

Modeling during freeze drying

Most authors analyzed the stability of encapsulated carote-noids by applying the Arrhenius model during freeze drying.However, Weibull model, Regression model, Higuchi model,Hixson-Crowell cube root law, and Korsmeyer Peppasmodel were also used to predict the shelf life of carotenoidsencapsulated using freeze drying. Kinetics parameters arehighly correlated with encapsulating materials, sources ofcarotenoids, and storage conditions (Table 5). Higher tem-peratures resulted in a higher degradation rate and higherhalf-life than lower temperature for all encapsulated carote-noids (Table 5). Tang and Chen (2000; Chen and Tang1998) encapsulated lutein from carrot using sucrose and gel-atin and showed that the degradation rate constant of luteinwas lower than those of a-and b-carotene because of theformation of lutein and gelatin complex. Activation energywas related to the amounts of carotenoids and encapsulatingmaterials. First order kinetic reaction for encapsulated caro-tenoids was described by the most of the authors using theArrhenius model. However, Weibull model and Regressionmodel were also fitted to measure the kinetic parameters forencapsulated carotenoids. However, Sen Gupta and Ghosh(2015) used Zero order, First order, Higuchi model, Hixson-Crowell cube root law, and Korsmeyer-Peppas model wereused for determination of the controlled release kineticsfrom encapsulated crude palm oil using isabgol fiber. SenGupta and Ghosh (2015) also confirmed fitting of five mod-els that followed a non-Fickian diffusion pattern for encap-sulated crude palm oil. Moreover, Higuchi model showedthe best linearity due to higher R2 value. Therefore, differentmodels could be applied to obtain information regarding thedegradation of carotenoids encapsulated using freeze drying.

Effects of encapsulated carotenoids onbioavailability

Bioavailability of any bioactive compounds refers to the pro-portion of a particular nutrient that is digested, absorbed,and metabolized via the normal pathways (Gul et al. 2016).A number of factors are responsible for stimulating or limit-ing the bioavailability of carotenoids (Ribeiro et al. 2008;Bohn 2008). Carotenoids need to be released mechanicallyor enzymatically from the food matrix to be bioavailable.Carotenoids have limited water solubility, and they need tobe incorporated into lipid droplets. The low bioavailabilityof carotenoids from natural sources is thought to be eitherdue to their existence as crystals or location within proteincomplexes that cannot be properly released in the GI tractduring digestion (Williams, Boileau, and Erdman 1998). Useof coating material during processing of carotenoids enhan-ces the stability and helps in controlled released of thesebioactive compounds in the human body (Gul et al. 2016).A number of studies reported that microencapsulation sig-nificantly affects the bioavailability of carotenoids in bothTa

ble4.

Continued.

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

DE.25

DEalso

used

asreference.

K 15G

lc(t>

t c)¼

0.022,

E a¼7.71

(Kcal/m

ol),t (1

/2)¼

30.7±1.6(weeks)

K 15G

al(t<

t c)¼

0.112,

E a¼12.10(Kcal/m

ol),t (1

/2)¼6.2±0.8(weeks)

K 15G

al(t>

t c)¼

0.024,

E a¼7.65

(Kcal/m

ol),t (1

/2)¼

28.5±1.5(weeks)

K 15Lac(t<

t c)¼

0.117,

E a¼12.02(Kcal/m

ol),t (1

/2)¼

5.9±0.8(weeks)

K 15Lac(t>

t c)¼

0.021,

E a¼7.75

(Kcal/m

ol),t (1

/2)¼

33.1±2.7(weeks)

K 4Glc(t<

t c)¼

0.047,

E a¼17.07(Kcal/m

ol),t (1

/2)¼14.7±1.3(weeks)

K 4Glc(t>

t c)¼

0.008,

E a¼13.15(Kcal/m

ol),t (1

/2)¼87.2±3.4(weeks)

K 4Gal(t<

t c)¼

0.057,

E a¼17.43(Kcal/m

ol),t (1

/2)¼

12.1±1.3(weeks)

K 4Gal(t>

t c)¼

0.010,

E a¼13.31(Kcal/m

ol),t (1

/2)¼

71.0±4.2(weeks)

K 4Lac(t<

t c)¼

0.049,

E a¼17.53(Kcal/m

ol),t (1

/2)¼

14.2±1.4(weeks)

K 4Lac(t>

t c)¼

0.009,

E a¼13.35(Kcal/m

ol),t (1

/2)¼

75.4±3.4(weeks)

K¼Degradatio

nrate

constants,t 1/2¼half-life,

E a¼Activationenergy,/t¼enthalpy

relaxatio

ndu

ringtim

e,DH1¼totalenthalpy,DHrelax¼enthalpy

relaxatio

ndu

ringagingtim

e,DCp

¼heat

capacity

changing

atthe

glasstransitio

ntemperature

(Tg),Ta

¼Ag

ingtemperature,sandb

valueob

tained

from

STAT

ISTICA

TM,OSA

1,OSA

2,OSA

3¼diffe

rent

mod

ified

starch,s F¼lifetim

e,s s¼slow

decaycompo

nents,

t S¼delaytim

e,sD

¼lifetim

eun

derdark

cond

ition

.

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 17

in-vitro and in-vivo studies (Roman, Burri, and Singh 2012;Han et al. 2008; Donhowe and Kong 2014; Aissa et al.2012). The higher water dispensability of carotenoids resultsin higher bioavailability (Thurmann et al. 2002).Microencapsulation of carotenoids promotes their bioavail-ability (Soukoulis and Bohn 2015) by a number of ways:

a. increasing the stability against isomerization and deg-radation due to different factors,

b. improving solubility resulting in increased bioaccessibil-ity, and

c. helping targeted release kinetics.

Effects of encapsulated carotenoids in vitro studies

In vitro intestinal digestion of b-carotene encapsulated byalginate and chitosan was investigated in some studies (Hanet al. 2008; Roman, Burri, and Singh 2012), proving that, it isnot necessarily correlated with complete transfer of b-caroteneinto micelle phase during intestinal digestion. The authorsfound that the total concentration of b-carotene in the micellecell was negligible. This could be due to inhibition of micelleformation by soluble fiber alginate. These results necessitatedfurther studies of micelle formation to obtain a clear under-standing for bioavailability of microencapsulated b-carotene.Encapsulated b-carotene also showed high resistance to gastricpH (Han et al. 2008). This resistance of encapsulated beadsduring the transit through stomach may be because of theexistence of an external layer of chitosan-alginate coacervate.The release behavior of encapsulated b-carotene showed effi-cient controlled release and maintained maximum release per-centage. This may be due to minimal water absorption of theencapsulating polymers, which enhance swelling and result inno hydrophobic interaction between cohesive forces withinthe polymeric matrix. Microencapsulating agents can protectthe micronutrients from enzymatic and acidic environmentsduring the release condition, as well as result in controlledrelease mechanism of encapsulated micronutrients throughgastrointestinal transit (Tiena, Ispas-Szaboa, and Mateescu2003). Similar results were found in isabgol fiber (Phylliumhusk) encapsulated carotenoids from the crude palm oil,showing that fibrous coated carotene regulated effectiverelease (Sen Gupta and Ghosh 2015).

Effects of encapsulated carotenoids in vivo studies

The in vivo studies of gum arabic microencapsulated b-caro-tene by spray drying and pure b-carotene activity againstgenotoxicity showed that the microencapsulated b-carotenehad higher potential, as compared to pure b-carotenebecause microencapsulation process induces the bioavailabil-ity of carotenoids (Aissa et al. 2012). Thus, the encapsulatedb-carotene maintained the anti-oxidative properties. Thephysicochemical properties and bioavailability of luteinmicroencapsulation showed that encapsulated lutein showedmore bioavailability, compared to the commercial referencesample (Zhang et al. 2015). Matrix of modified food starchwas used as wall material for preparing lutein

microencapsulated product. The enhanced bioavailabilitywas because the high solubility of wall materials induces theaqueous solubility of lutein. The results under the conditionof dissolution test, LM dissolution rate was very high, whichmay be because bioavailability of LM was not restricted bydissolution behavior. Similar findings reported that encapsu-lated carotenoids enhance their solubility and release duringdigestion (Wang and Bohn 2012). Encapsulated carotenoidsare more easily delivered into the cellular compartments,resulting in better bioavailability.

Advantages of the encapsulated carotenoids andcompared to the non-encapsulated carotenoids inthe food system

It is important to determine whether the encapsulated caro-tenoids are stable or not in the food system. However, thereare very few studies of encapsulated carotenoids in the foodsystems. Synthetic trans b-carotene, encapsulated withalmond gum and gum arabic, was used to prepare cake. Theresults showed that cake made with almond gum had sig-nificantly higher a� value than cake made with gum arabic(Mahfoudhi and Hamdi 2015). These results might be dueto higher protection of b-carotene on encapsulation withalmond, as compared to encapsulation with gum arabic.Another study reported by Kha et al. (2015), who developedyogurt, pasteurized milk, and cake with encapsulated gac oilusing whey protein concentrate and gum arabic. The resultsshowed that incorporation with encapsulated gac oil prod-ucts color was unchanged, as well as b-carotene and lyco-pene was slightly decreased during storage. The authorsreported that auto-oxidation, photo-oxidation, and photo-isomerization were responsible for changes in the b-caroteneand lycopene through the storage period. Coronel-Aguileraand Martin-Gonzalez (2015) produced b-carotene spraydried powder using maltodextrin and sodium casemate, fol-lowed by fluidized bed coater and applied to a yogurt systemand also compared with commercial peach yogurt. Thesestudies revealed that the total color value of yogurt madewith encapsulated b-carotene was comparable with thestandard value and also stable in acidic media for fourweeks during storage at 4 �C. Food matrix (pudding andyogurt) was manufactured using encapsulated b-carotenewith maltodextrin, water-dispersible powder, and chitosan-alginate beds (Donhowe et al. 2014). Food matrix signifi-cantly affected in terms of release of b-carotene duringdigestion and incorporation into the micelle phase. Yogurtmade with encapsulated b-carotene showed lower releaserate of b-carotene and content of b-carotene in the micellephase than those of pudding made with encapsulatedb-carotene. This might be due to the pH of the food matrixand coagulation of the food matrix, as well as protein com-position of the food matrix (Donhowe et al. 2014).

Conclusions

In this review, we discussed the encapsulation of carotenoidsusing various encapsulating agents through spray and freeze

18 J.-B. EUN ET AL.

Table5.

Degradatio

nkineticsmod

elingof

encapsulated

caroteno

idsdu

ringfreeze

drying

.

Sourcesof

caroteno

ids

Operatin

gcond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Carrot

pulp

Storageat

(4� C

dark,2

5� C

dark,4

5� C

dark

and

25� C

light)

Sucroseandgelatin

First-orderkinetic

mod

elLutein

K 4� C

(dark)

¼0.004(day

�1 )

K 25�C(dark)

¼0.006(day

�1 )

K 45�C(dark)

¼0.009(day

�1 )

K 25�C(ligh

t)¼

0.013(day

�1)

a-Carotene

K 4� C

(dark)

¼0.013(day

�1 )

K 25�C(dark)

¼0.020(day

�1 )

K 45�C(dark)

¼0.032(day

�1 )

K 25�C(ligh

t)¼

0.039(day

�1)

b-Carotene

K 4� C

(dark)

¼0.015(day�

1 )K 2

5�C(dark)

¼0.024(day

�1 )

K 45�C(dark)

¼0.037(day

�1 )

K 25�C(ligh

t)¼

0.043(day

�1)

Tang

andCh

en(2000)

Carrot

pulp

waste

Storageat

(4� C

dark,2

5� C

dark,4

5� C

dark

and

25� C

light)

Sucroseandgelatin

First-orderkinetic

mod

el,

Lutein

K 4� C

(dark)

¼0.005(day

�1 )

K 25�C(dark)

¼0.008(day

�1 )

K 45�C(dark)

¼0.011(day

�1 )

K 25�C(ligh

t)¼

0.015(day

�1)

a-Carotene

K 4� C

(dark)

¼0.014(day

�1 )

K 25�C(dark)

¼0.026(day

�1 )

K 45�C(dark)

¼0.043(day

�1 )

K 25�C(ligh

t)¼

0.049(day�

1 )

b-Carotene

K 4� C

(dark)

¼0.018(day�

1 )K 2

5�C(dark)

¼0.031(day�

1 )K 4

5�C(dark)

¼0.050(day�

1 )K 2

5�C(ligh

t)¼

0.058(day

�1)

Chen

andTang

(1998)

Sourcesof

caroteno

ids

Storagecond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Brow

nseaw

eed

(Phaeoph

yceae)

Storageat

(28,

45and65

� Cin

dark)

Maltodextrin

and

Tween80

First-orderkinetic

mod

el.

lnC¼

lnC0

–k(t)

Arrheniusmod

elk¼Ae

�Ea/R/T

Trans-fucoxanthin

a�(therm

o-labile

caroteno

ids)

K 28�C¼

0.0356

(day

�1 )

K 45�C¼

0.1454

(day

�1 )

K 65�C¼

0.6349

(day

�1 )

t 1/2( 28�C)¼

63(days)

t 1/2( 45�C)¼

15(days)

t 1/2( 65�C)¼

4(days)

Ea¼

15.73(Kcal/m

ol)

b�(pheop

hytin

aandchloroph

yllc)

K 28�C¼

0.0659

(day

�1 )

K 45�C¼

0.3518

(day

�1 )

K 65�C¼

2.0331

(day

�1 )

t 1/2( 28�C)¼

88(days)

t 1/2( 45�C)¼

16(days)

t 1/2( 65�C)¼

3(days)

Ea¼

18.72(Kcal/m

ol)

Indraw

atie

tal.(2015)

Crud

epalm

oil

Storageat

(30� C)for30

days

Isabgo

lfiber

(Psyllium

husk)

zero

order(ko),first

order(k1)

Higuchi

mod

el(kH),

Hixson-Crow

ell

cube

root

law(kHc)

Zero

Order

k o(m

g�h�1)¼

2.2025

Firstorder

SenGup

taand

Gho

sh(2015).

(continued)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 19

Table5.

Continued.

Sourcesof

caroteno

ids

Operatin

gcond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

andKorsmeyer

Pepp

asmod

el(K

KP)

k 1(h

�1)¼

0.267

Higuchi

k H(h

�1/2 )¼

32.8

Hixson-Crow

ell

kHc(h

�1/3 )¼

0.347

Korsmeyer-Peppas

K KP(h

�n)¼

3.418

Turm

eric

Storageat

25� C

for8weeks

gum

arabicmaltodextrin

mod

ified

starch

Pseudo

-firstorderkinetics.

Regression

mod

elCu

rcum

inMaltodextrin

(75%

)andmod

ified

starch

(25%

)ln(CR)

¼4.61–0.088(t)

Gum

arabic

ln(CR)

¼4.62–0.048(t)

gum

Arabic(33%

),maltodextrin

(33%

)and

mod

ified

starch

(33%

)ln(CR)

¼4.58-0.051(t)

Cano

-Higuita,M

alacrid

a,andTelis

(2015)

Tomatopu

lpwaste

Storageat

(4,2

5and35

� C)

for35

days

gelatin

andpo

ly(c-

glutam

icacid)

Firstorderkinetics.

L¼L0

�[exp

(-kt) ]

Arrheniusmod

elln(k)¼

–Ea/R(T/

1)þ

ln(A)

Forcislycopene

L(4�C)¼

47.30[–exp(0.0062)t],K

( 4� C)¼

6.20

�10

�3(days�

1 )L(25

� C)¼

46.13[–exp(0.0133)t],K

( 25�C)¼

1.33

�10

�3(days-1 )

L(35

� C)¼

44.07[–exp(0.0199)t],K

( 35�C)¼

1.99

�10

�3(days1)

E a¼

26.89(KJ/mol)

Fortranslycopene

L(4�C)¼

89.88[–exp(0.0077)t],K

( 4� C)¼

7.70

�10

�3(days�

1 )L(25

� C)¼

86.06[–exp(0.0181)t],K

( 25�C)¼

1.81

�10

�3(days1)

L(35

� C)¼

80.55[–exp(0.0247)t],K

( 35�C)¼

2.47

�10

�3(days1)

E a¼

26.37(KJ/mol)

Fortotallycop

ene

L(4�C)¼

137.15[–exp(0.0071)t]K(

4�C)¼

7.17

�10

�3(days�

1 )L(25

� C)¼

132.18[–exp(0.0163)t],K(

25� C)¼

1.63

�10

�3(days�

1 )L(35

� C)¼

124.56[–exp(0.0229)t],K(

35� C)¼

2.29

�10

�3(days�

1 )E a¼

26.52(KJ/mol)

Chiu

etal.(2007).

Pure

transb-carotene

Storageat

250 C

for

seventeenweeks

Maltodextrin

25DE

First-orderkinetic

mod

elArrheniusmod

elK 2

5DE(t<t c)¼

0.110±0.008,

E a¼

12.64(Kcal/

mol),t (1

/2)¼

6.3(weeks)

K 25D

E(t>t c)¼

0.020±0.004,

E a¼

8.74

(Kcal/

mol),t (1

/2)¼

34.5

(weeks)

Desob

ry,N

etto,and

Labu

za(1997)

Trans-b-carotene

Storageat

25� C

under

diffe

rent

relativehu

midities

Almon

dandgu

marabic

First-orderkinetic

mod

elWeibu

llmod

elln[(R

-R 1

)/(R

0-

R 1)]¼

-k Dt

ForAlmon

dgu

mK D

(RH

10%)¼

0.0178

±0.0025;R

1(RH

10%)¼

58.4±4

K D(RH

45%)¼

0.025±0.0013;R

1(RH

45%)¼

6.53

±1.2

K D(RH

80%)¼

matrix

collapsed;R

1(RH

80%)¼

matrix

collapsed

ForGum

arabic

K D(RH

10%)¼

0.024±0.0015;R

1(RH

10%)¼

Mahfoud

hiand

Ham

di(2015)

20 J.-B. EUN ET AL.

55.08±3.2

K D(RH

45%)¼

0.0397

±0.002;

R 1(RH

45%)¼

3.99

±1.1

K D(RH

80%)¼

-;R 1

(RH

80%)¼

-

b-carotene

Storageat

25� C

under

diffe

rent

relativehu

midities

Mannitol–ph

osph

ate

matrices

(from

solutio

nsprepared

with

phosph

atebu

ffer

50mM

pH7.4)

First-orderkinetic

mod

elWeibu

llmod

elln[(R

-R 1

)/(R

0-

R 1)]¼

-k Dt

K D(RH

11%)¼

0.035±0.005;

R 1(RH

11%)¼

60±3

K D(RH

44%)¼

0.081±0.01;R

1(RH

45%)¼

2.20

±1

K D(RH

75%)¼

matrix

collapsed;R

1(RH

75%)¼

matrix

collapsed

Sutter,B

uera.and

Elizalde

(2007)

Transb-carotene

Storageat

(10� C

dark,2

5� C

dark,and

UVlight)

Nativestarch,6

DE

starch,1

2DEstarch

First-orderkinetic

mod

elln

(Ct/C

0)¼

±kt

t 1/2¼

0.693/k

Weibu

llmod

elln

(Ct/C

0)¼

-btn

Forna

tive

starch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.048±0.001(day�

1 )K 2

5�C(dark)

¼0.076±0.006(day�

1 )K 2

5�C(UVlight)¼

0.149±0.006(day

�1)

Weibu

llmod

elb 1

0�C(dark)

¼0.059±0.015

b 25�C(dark)

¼0.010±0.004

b 25�C(UVlight)¼

0.246±0.058

n 10�C(dark)

¼0.952±0.081

n 25�C(dark)

¼1.624±0.130

n 25�C(UVlight)¼

0.821±0.070

For6DEstarch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.030±0.002(day�

1 )K 2

5�C(dark)

¼0.031±0.001(day�

1 )K 2

5�C(UVlight)¼

0.088±0.004(day

�1)

Weibu

llmod

elb 1

0�C(dark)

¼0.079±0.013

b 25�C(dark)

¼0.050±0.007

b 25�C(UVlight)¼

0.177±0.027

n 10�C(dark)

¼0.695±0.053

n 25�C(dark)

¼0.845±0.046

n 25�C(UVlight)¼

0.771±0.049

For12

DEstarch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.014±0.001(day�

1 )K 2

5�C(dark)

¼0.017±0.001(day�

1 )K 2

5�C(UVlight)¼

0.026±0.001(day

�1)

Weibu

llmod

elb 1

0�C(dark)

¼0.026±0.009

b 25�C(dark)

¼0.033±0.003

b 25�C(UVlight)¼

0.014±0.006

n 10�C(dark)

¼0.821±0.108

n 25�C(dark)

¼0.786±0.036

n 25�C(UVlight)¼

1.171±0.134

Spadaet

al.(2012)

Pure

b-carotene

Storageat

(10� C

dark,2

5� C

dark,and

UVlight)

Nativestarch,6

DE

starch,1

2DEstarch

First-orderkinetic

mod

elln

(Ct/C

0)¼

±kt

t 1/2¼

0.693/k

Weibu

llmod

elln

(Ct/C

0)¼

-btn

Forna

tive

starch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.048±0.001(day�

1 )K 2

5�C(dark)

¼0.076±0.006(day�

1 )K 2

5�C(UVlight)¼

0.149±0.006(day

�1)

Spadaet

al.(2012)

(continued)

CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 21

Table5.

Continued.

Sourcesof

caroteno

ids

Operatin

gcond

ition

sCarrieragents

Kinetic

order

Mathematical

mod

elKinetic

parameters

References

Weibu

llmod

elb 1

0�C(dark)

¼0.059±0.015

b 25�C(dark)

¼0.010±0.004

b 25�C(UVlight)¼

0.246±0.058

n 10�C(dark)

¼0.952±0.081

n 25�C(dark)

¼1.624±0.130

n 25�C(UVlight)¼

0.821±0.070

For6DEstarch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.030±0.002(day�

1 )K 2

5�C(dark)

¼0.031±0.001(day�

1 )K 2

5�C(UVlight)¼

0.088±0.004(day

�1)

Weibu

llmod

elb 1

0�C(dark)

¼0.079±0.013

b 25�C(dark)

¼0.050±0.007

b 25�C(UVlight)¼

0.177±0.027

n 10�C(dark)

¼0.695±0.053

n 25�C(dark)

¼0.845±0.046

n 25�C(UVlight)¼

0.771±0.049

For12

DEstarch

First-orderkinetic

mod

elK 1

0�C(dark)

¼0.014±0.001(day�

1 )K 2

5�C(dark)

¼0.017±0.001(day�

1 )K 2

5�C(UVlight)¼

0.026±0.001(day

�1)

Weibu

llmod

elb 1

0�C(dark)

¼0.026±0.009

b 25�C(dark)

¼0.033±0.003

b 25�C(UVlight)¼

0.014±0.006

n 10�C(dark)

¼0.821±0.108

n 25�C(dark)

¼0.786±0.036

n 25�C(UVlight)¼

1.171±0.134

Pure

b-carotene

Storageat

25� C

under

diffe

rent

relativehu

midities

Maltodextrin

,gelatin,

andgu

marabic

First-orderkinetic

equatio

nof

fractio

nalretentio

n.Weibu

llmod

elln[(R

-R 1

)/(R

0-

R 1)]¼

k Dt

Formaltodextrin

K D(RH

11%)¼

0.08

±0.02;R

1(RH

11%)¼

44±3

K D(RH

44%)¼

0.97

±0.05;R

1(RH

44%)¼

41±1

K D(RH

75%)¼

1.4±0.05;R

1(RH

11%)¼

35±4

K D(RH

92%)¼

2.2±0.1;

R 1(RH

92%)¼

0Formaltodextrin

:gelatin

(200:

100g/kg

�1)

K D(RH

11%)¼

0.08

±0.02;R

1(RH

11%)¼

44±3

K D(RH

44%)¼

0.97

±0.05;R

1(RH

44%)¼

41±1

K D(RH

75%)¼

1.4±0.05;R

1(RH

11%)¼

35±4

K D(RH

92%)¼

2.2±0.1;

R 1(RH

92%)¼

0Formaltodextrin

andgu

marabic(200:1

00g/

kg�1

K D(RH

11%)¼

0.08

±0.02;R

1(RH

11%)¼

44±3

K D(H

44%)¼

0.97

±0.05;R

1(RH

44%)¼

41±1

K D(RH

75%)¼

1.4±0.05;R

1(RH

11%)¼

35±4

K D(RH

92%)¼

2.2±0.1;

R 1(RH

92%)¼

Ramon

edaet

al.(2011)

K¼Degradatio

nrate

constants,t 1/2¼

half-life,

E a¼

Activationenergy,CR

¼curcum

inretention,

L¼degradationrate

equatio

nt¼

first

phase,

t c¼

second

phase,

bandnaredepend

entcoefficients,R 1

¼asym

ptotic

value,K D

¼rate

constant,R

0andR¼

percentage

ofb-caroteneretentionat

zero

timeandtim

et.

22 J.-B. EUN ET AL.

drying of different food materials. Moreover, we also eluci-dated the impact of various encapsulating agents on carote-noids from various sources, as well as degradation kineticsof encapsulated carotenoids during processing and storage.Most of the studies performed to produce encapsulated car-otenoids using various encapsulating agents through sprayand freeze drying. Among these, maltodextrins are com-monly used as encapsulating agents and spray drying ismost suitable drying methods for encapsulation. However,several studies can be applied in near future:

� How to improve encapsulated carotenoids absorp-tion efficiency.

� Absorption mechanisms of encapsulated carotenoids.� Which encapsulating agent is more involved in bioavali-

bility of encapsulated carotenoids during digest-ive process?

� Effects of encapsulated carotenoids on human healthespecially in the treatment of specific disorder.

Funding

The authors are grateful for financial support received from BK 21Plus Program, Graduate School of Chonnam National University,Gwanju, South Korea.

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